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Method for preparing palladium/carbon catalyst for hydrogenation

A carbon catalyst and catalyst technology, which is applied in catalyst activation/preparation, organic compound preparation, physical/chemical process catalysts, etc., can solve the problems of difficult uniform distribution of supported activated carbon, strong uncertain negative effects, and damage to catalyst performance, etc. Ease of environmental protection, long service life, high microcrystal content

Inactive Publication Date: 2005-11-23
SINOPEC SHANGHAI PETROCHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because hydrogen peroxide itself is also oxidizing, it can oxidize the surface groups of activated carbon, which will change the surface physical and chemical properties of the support, that is, change the surface group structure of the support, which has a strong uncertain negative impact and will damage the catalyst. Other properties, such as palladium loading strength, catalyst life, selectivity, etc.
U.S. Patent No. 4,476,242 proposes to use organic solvents such as methanol or pyridine to prepare impregnation solutions containing Pd compounds. It is said that this is also very effective in preventing the migration of Pd and grain growth, but the production process uses methanol or pyridine, which is harmful to the human body. Harmful organic compounds are unfavorable in terms of environmental protection or labor protection
In addition, there is a patent report to convert the chloropalladium acid solution into a palladium colloid by adjusting the pH value, which is said to prevent the reducing groups on the surface of the activated carbon from directly reducing Pd ions to zero-valent metal Pd, but the colloid is not stable. , it is difficult to distribute evenly on the carrier activated carbon, which will also affect the dispersion of Pd

Method used

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  • Method for preparing palladium/carbon catalyst for hydrogenation
  • Method for preparing palladium/carbon catalyst for hydrogenation
  • Method for preparing palladium/carbon catalyst for hydrogenation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] 100 grams of 4-8 mesh, specific surface 800-1800m 2 / g coconut shell activated carbon is washed with 0.4N nitric acid at 80°C, then washed with water until neutral, and dried at 120°C for 2 to 8 hours for later use.

[0038] The preparation of Pd solution, get 3.4 grams of 15.0wt% chloropalladium acid solution, add deionized water to 40 milliliters, then add 0.78 milliliters of 5wt% 8-hydroxyquinoline acidic aqueous solution, and add deionized water to prepare Pd solution 60ml. After the Pd solution is stable for 10 to 200 minutes, the above treated activated carbon is impregnated with the Pd solution for 4 hours to obtain a catalyst precursor. Aging of the catalyst precursor for 24 hours, using 20 grams of 5wt% hydrazine hydrate and 200 grams of pure water to prepare a reducing solution, immersing the catalyst precursor in the reducing solution for 2 to 4 hours, then washing with pure water to neutrality and drying Catalyst products are obtained.

Embodiment 2~24

[0040] Select different Pd-containing compounds and complexing agents to prepare the Pd solution, and the rest are the same as in Example 1, the specific Pd-containing compound, the content of the Pd-containing compound (in Pd) in the Pd solution, the specific complexing agent and complexing agent The molar ratio with Pd is listed in Table 1.

Embodiment 25~30

[0042] Different Pd-containing compounds and complexing agents were selected to prepare the Pd solution. After the Pd solution was stable for 10-200 minutes, the Pd solution was sprayed on activated carbon to obtain a catalyst precursor, and the rest was the same as in Example 1.

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PUM

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Abstract

This invention relates to a method for preparing a hydrogenation palladium or carbon catalyst. The catalyst uses the particles or shaping active carbon as the carrier, loading active component metal Pd, wherein the Pd content is 0.2-5wt%. The preparing method comprises the following steps: a) acid cleaning the carrier active carbon; then flushing with water until neutral; drying; b) preparing Pd solution with water-soluble Pd compound and a complex builder; using Pd solution to immerse or spray the carrier active carbon, loading the Pd compound on the active carbon and then getting the catalyst prosoma, wherein the Pd compound content is 15-20wt% computed by Pd, the molecular ratio of complex builder and Pd is (0.01-1):1, the complex builder is any one from 8-bioquin, 2,3,4-trihydroxy-4-sulfonic acid azobenzene, ortho phenanthroline, o-aminophenol, o-hydroxybenzoic acid sodium or salicylaldehyde benzaldoxime; c) aging the catalyst prosoma, then deacidizing and getting the catalyst.

Description

technical field [0001] The invention relates to a preparation method of a supported palladium / carbon catalyst for hydrogenation reaction, in particular to a preparation method of a supported palladium / carbon catalyst for refining crude terephthalic acid through selective hydrogenation reaction. Background technique [0002] The supported palladium / carbon catalyst is mainly used for the selective hydrogenation of unsaturated organic matter, especially for the purification of crude terephthalic acid. Impurities such as p-carboxybenzaldehyde (4-CBA) in crude terephthalic acid are After the hydrogen is transformed into other compounds, it can be separated and purified by crystallization. Because the palladium / carbon catalyst usually adopts a single active component, its improvement research has always focused on the structure of the support and the distribution of metal Pd on the support in the prior art, and this will indeed have a great impact on the performance of the catalys...

Claims

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Application Information

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IPC IPC(8): B01J23/44
Inventor 钱斌陈大伟吴征
Owner SINOPEC SHANGHAI PETROCHEMICAL CO LTD
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